EP1095690A1 - Verfahren zum Reinigen eines Gases und entsprechende Vorrichtung - Google Patents

Verfahren zum Reinigen eines Gases und entsprechende Vorrichtung Download PDF

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Publication number
EP1095690A1
EP1095690A1 EP00402895A EP00402895A EP1095690A1 EP 1095690 A1 EP1095690 A1 EP 1095690A1 EP 00402895 A EP00402895 A EP 00402895A EP 00402895 A EP00402895 A EP 00402895A EP 1095690 A1 EP1095690 A1 EP 1095690A1
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EP
European Patent Office
Prior art keywords
adsorber
auxiliary
main
gas
adsorbers
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EP00402895A
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English (en)
French (fr)
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EP1095690B1 (de
Inventor
Alain Guillard
Patrick Le Bot
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B01D53/047—Pressure swing adsorption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B01D53/0462—Temperature swing adsorption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/104—Alumina
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/106—Silica or silicates
    • B01D2253/108—Zeolites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/116—Molecular sieves other than zeolites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/504—Carbon dioxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/80—Water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
    • B01D2259/40043—Purging
    • B01D2259/4005—Nature of purge gas
    • B01D2259/40056—Gases other than recycled product or process gas
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
    • B01D2259/40058—Number of sequence steps, including sub-steps, per cycle
    • B01D2259/4006—Less than four
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
    • B01D2259/40077—Direction of flow
    • B01D2259/40081—Counter-current
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/403—Further details for adsorption processes and devices using three beds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/404—Further details for adsorption processes and devices using four beds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/414—Further details for adsorption processes and devices using different types of adsorbents
    • B01D2259/4141—Further details for adsorption processes and devices using different types of adsorbents within a single bed
    • B01D2259/4145—Further details for adsorption processes and devices using different types of adsorbents within a single bed arranged in series
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/414—Further details for adsorption processes and devices using different types of adsorbents
    • B01D2259/4141—Further details for adsorption processes and devices using different types of adsorbents within a single bed
    • B01D2259/4145—Further details for adsorption processes and devices using different types of adsorbents within a single bed arranged in series
    • B01D2259/4146—Contiguous multilayered adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26—Drying gases or vapours
    • B01D53/261—Drying gases or vapours by adsorption
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2

Definitions

  • the present invention relates to a process for purifying a gas by adsorption of a first impurity and a second impurity, of the type in which is used cyclically several adsorbers selectively in phase adsorption and regeneration phase.
  • the invention applies, for example, to the purification of air with a view to its distillation.
  • a purification device comprising two identical adsorbers, the operation of which is alternating, i.e. one is in the adsorption phase while the other is in the adsorption phase of regeneration.
  • An object of the invention is to provide a method of the aforementioned type which allows, in particular, to further reduce the costs of manufacturing or operation of an air distillation installation in which the process is implemented.
  • the invention relates to a process of the aforementioned type, characterized in that at least two main adsorbers are used and at least one auxiliary adsorber, in that, for at least a first stage, the gas is purified by adsorbing the two impurities by passing through minus a first of the main adsorbers without going through a first auxiliary adsorber, and simultaneously regenerates the second one in parallel main adsorber and the or each auxiliary adsorber, then for a second step, at least part of the gas flow is purified by adsorption of the two impurities by passing in series through the first main adsorber and in the first auxiliary adsorber.
  • the invention further relates to a device for purifying a gas for the implementation of a process as defined above, characterized in that it includes a gas supply line to be purified, a gas evacuation line purified, a regeneration gas supply line, an evacuation line for the regeneration gas, at least two main adsorbers and at least one auxiliary adsorber, the main adsorbers comprising a lining adsorption of the first and second impurities and each auxiliary adsorber comprising an adsorption lining of at least the second impurity, and that the device further comprises first connection means, to connect the main adsorbers to the purified gas discharge line without passing through the auxiliary adsorber or without passing through any of the adsorbers auxiliary, second connection means, for connecting in series each main adsorber with an auxiliary adsorber, and thirds connection means, for connecting the or each adsorber in parallel auxiliary and at least one main adsorber to the gas supply line regeneration.
  • FIG. 1 represents a purification device 1 of an air distillation installation.
  • This device 1 can operate by variation of temperature and / or pressure.
  • This device 1 is intended to remove the majority of impurities, and in particular H 2 O and CO 2 , contained in a stream of compressed air at a pressure between 4 and 50 bar and brought by a line 2, to supply , via a line 3, a main heat exchange line then an air distillation apparatus.
  • the air distillation apparatus can be, for example, a medium pressure column of a double air distillation column.
  • the purification device 1 comprises two main adsorbers 5A and 5B identical, and two identical adsorbers 6A and 6B identical.
  • Each main adsorber 5A, B comprises a container or bottle 7A, B successively containing, in the adsorption direction which is vertical and directed upwards, a layer 8A, B of a material capable of adsorbing H 2 O , for example alumina, and a layer 9A, B of a material capable of adsorbing CO 2 , for example a molecular sieve.
  • the layer 8A, B has a thickness significantly greater than that of the layer 9A, B.
  • the material of the layers 8A, B and 9A, B can be similar. It is then a material capable of adsorbing the two impurities.
  • the material of the layer 8A, B generally represents between 60% and 100% of the adsorption lining loaded in the container 7A, B.
  • Each auxiliary adsorber 6A, B comprises a container 10A, B in which is disposed a single layer 11A, B of a material capable of absorbing CO 2 , for example the same material as that of the layers 9A and 9B.
  • the purification device 1 also comprises a certain number of connecting pipes and valves whose arrangement will appear now when describing the process implemented in the device treatment 1.
  • This process is obtained by repeating a cycle comprising four successive steps I to IV.
  • stage I the main adsorber 5A is in the adsorption phase, while the main adsorber 5B and the auxiliary adsorbers 6A and 6B are in the regeneration phase.
  • the air from line 2 is then supplied by a valve 13A open in the main adsorber 5A.
  • the air successively passes through layer 8A, where the H 2 O is fully adsorbed, then through layer 9A, where the CO 2 is fully adsorbed.
  • the purified air that is to say drawn and decarbonated, is then returned via two valves 15A and 16A open directly to line 3, that is to say without passing through another adsorber.
  • This residual nitrogen circulates in the adsorbers 5B, 6A and 6B in the sense of regeneration, i.e. in the opposite direction to the sense of adsorption, by ensuring the regeneration of these adsorbers including layers 8B, 9B, 11A and 11B were significantly saturated in a previous cycle.
  • the residual nitrogen transporting the desorbed H 2 O and the CO 2 is then returned, on the one hand, to the auxiliary adsorbers 6A and 6B via open valves 26A and 26B, and on the other hand, to the main adsorber 5B via an open valve 30B, to a discharge line 32.
  • step I is continued until the layer 9A is substantially saturated with CO 2 and the adsorber 6A is regenerated.
  • step II the valves 16A, 20A and 26A are closed and the air, drawn by the layer 8A and leaving the main adsorber 5A, is returned to the auxiliary adsorber 6A by an open valve 34A. Air purification is then continued by adsorption of CO 2 in layer 11A. The desiccated and decarbonated air leaving the auxiliary adsorber 6A is then returned via a valve 36A open directly to line 3.
  • the auxiliary adsorber 6A is therefore in phase adsorption to purify the air in series with the main adsorber 5A.
  • step II The main adsorbers 5B and auxiliary 6B are, as in step I, regenerated in parallel. This step II continues until the layer 8A is substantially saturated with H 2 O or until the layer 11A is substantially saturated with CO 2 , and the main adsorber 5B is regenerated.
  • step III the adsorber 5B is in the adsorption phase, alone ensuring the purification of the air from line 2.
  • the adsorbers 5A, 6A and 6B are regenerated in parallel.
  • the journey of air and residual nitrogen can be deduced from the description of step I by reversing the suffixes A and B.
  • step III continues until the layer 9B is substantially saturated with CO 2 and the adsorber 6B is regenerated.
  • stage IV the main adsorbers 5B and auxiliary 6B purify the air from line 2 in series, the main adsorbers 5A and auxiliary 6A being in the regeneration phase.
  • the path of air and nitrogen can be deduced from the description of step II by reversing the suffixes A and B.
  • Step IV continues until the adsorber 5A is regenerated and the layer 8B is substantially saturated with H 2 O or that the layer 11B is substantially saturated with CO 2 .
  • the main adsorbers 5A and 5B are regenerated during half the cycle, but the auxiliary adsorbers 6A and 6B are regenerated during three stages of the cycle, namely stages I, III and IV for the adsorber auxiliary 6A and steps I, II and III for the adsorber 6B. Due to the time of relatively long regeneration of these auxiliary adsorbers 6A and 6B, the flow of residual nitrogen, necessary for regeneration and circulating in line 18, is reduced. Consequently, the pressure losses upstream of line 18 are also reduced.
  • the air circulating in the auxiliary adsorbers 6A and 6B is drawn. There is therefore no H 2 O to desorb adsorbers 6A and 6B.
  • the regeneration direction in the auxiliary adsorbers 6A and 6B can be directed upwards.
  • the direction of adsorption in the adsorbers 6A and 6B can therefore be directed downwards, which makes it possible to increase the speed of adsorption and therefore to reduce the dimensions of the containers 10A and 10B.
  • a compressor 38 is arranged between on the one hand the valves 15A and 15B, and on the other hand the valves 16A, 16B, 34A and 34B, to compress the air supplying line 3.
  • This compressor 38 is, for example, coupled to a turbine arranged in downstream of an intermediate outlet of the main heat exchange line of the air distillation installation, as described in applications FR-2 674 011, FR-2 701 553 and FR-2 723 184.
  • This compressor 38 compresses the purified air coming from the adsorber main 5A during stage I, the air drawn from the adsorber main 5A and supplying the auxiliary adsorber 6A during stage II, the air purified from the main adsorber 5B in step III, and the air drawing from the main adsorber 5B and feeding the adsorber auxiliary 6B during stage IV.
  • Tappings 39 and 40 arranged on the one hand between valves 15A and 15B and the compressor 38, and on the other hand between the compressor 38 and the valves 16A, 16B, 34A and 34B, allow to supply drawn air to devices not represented.
  • the adsorbers main 5A and 5B can be decarbonated in the auxiliary adsorbers 6A and 6B.
  • the compressor 38 is replaced by a turbine.
  • This turbine expands the purified air from the adsorber 5A during step I, the air drawn from the adsorber 5A and feeding the adsorber 6A during step II, the purified air coming from the adsorber 5B during step III, and the air drawn from the adsorber 5B and feeding the adsorber 6B during step IV.
  • the main and auxiliary adsorbers 5A and 6A are formed in the same container 40A provided with an intermediate partition interior 41A isolating the main adsorber 5A from the auxiliary adsorber 6A.
  • the auxiliary adsorber 6A surmounts the main adsorber 5A.
  • Partition 41A is domed and its concavity is directed towards the main adsorber 5A.
  • the structure of the main 5B and auxiliary 6B adsorbers is similar and is deduced from that of the adsorbers 5A and 5B by substituting the suffix B for the suffix AT.
  • This variant reduces the manufacturing cost of the adsorbers 5A, 5B, 6A and 6B and therefore the manufacturing cost of the distillation plant of air.
  • FIG. 4 illustrates another embodiment of a device air cleaning 1 distinguished from that of Figure 1 by the fact that the purification device 1 includes only one auxiliary adsorber 6.
  • the references of the elements relating to this auxiliary adsorber 6 will be the same than those concerning the adsorbers 6A and 6B of FIG. 1, the suffixes A or B being deleted.
  • the cycle of the purification process implemented by this device treatment plant 1 also comprises four stages I to IV described below.
  • stage I the main adsorber 5A is in the adsorption phase, while the main adsorbers 5B and auxiliary 6 are in the phase of regeneration.
  • the residual nitrogen from line 18 supplies the adsorber in parallel auxiliary 6, via valve 20 open, and main adsorber 5B, via valve 24B open.
  • the residual nitrogen, transporting the CO 2 and H 2 O accumulated in the layers 8B, 9B and 11 during a previous cycle and desorbed, is returned from the adsorbers 6 and 5B, via the valves 26 and 30B, open to line 32.
  • step I continues until the layer 9A is substantially saturated with CO 2 and the adsorber 5B is regenerated.
  • the air purification is ensured only by 5B adsorber.
  • the air from line 2 is then sent to the adsorber 5B via the valve 13B open.
  • the air drawn and decarbonated is then returned directly to line 3 via open valves 15B and 16.
  • valves 13A, 15A, 24A and 30A are closed so that the adsorber 5A is neither in the adsorption phase nor in the regeneration phase.
  • the auxiliary adsorber 6 is in the regeneration phase.
  • step II is continued until the layer 9B is substantially saturated with CO 2 and the auxiliary adsorber 6 is regenerated.
  • stage III the air from line 2 is sent via the valve 13A open to the main adsorber 5A where it is drawn. Then the air drawn is returned via open valves 15A and 34 to the adsorber auxiliary 6 which ensures the decarbonation of air. The purified air is then returned directly to line 3 via the open valve 36.
  • the adsorbers 5A and 6 are therefore in the adsorption phase to ensure in series the air purification of line 2.
  • Valves 13B, 15B, 24B and 30B are closed so that the adsorber auxiliary 5B is neither in the adsorption phase nor in the regeneration phase.
  • This step III continues until the layer 8A is substantially saturated with H 2 O.
  • the adsorbers 5B and 6 ensure the purification in series air.
  • the path of the residual air can be deduced from the description of step III substituting suffix B for suffix A.
  • the adsorber 5A is in the regeneration phase.
  • the residual nitrogen from line 18 is then sent via the open valve 24A to the main adsorber 5A.
  • the residual nitrogen carrying the H 2 O and the desorbed CO 2 is then returned via the valve 30A open to line 32.
  • Step IV continues until the layer 8B is substantially saturated with H 2 O.
  • the above process can purify a relatively large flow air with only three adsorbers 5A, 5B and 6. Therefore, the cost of manufacture of the air cleaning device 1, and therefore of the distillation installation of air, is relatively reduced.
  • a compressor 38 is arranged between on the one hand the valves 15A and 15B, and on the other hand the valves 16 and 34.
  • This compressor 38 corresponds to that of the variant of FIG. 3.
  • the compressor 38 ensures the compression of the drawn air and decarbonated from the main adsorbers 5A and 5B during steps I and II, and air drawn from the main adsorbers 5A and 5B and feeding the auxiliary adsorber 6 in steps III and IV.
  • the compressor 38 can also be replaced by a turbine.
EP00402895A 1999-10-25 2000-10-19 Verfahren zum Reinigen eines Gases und entsprechende Vorrichtung Expired - Lifetime EP1095690B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9913274 1999-10-25
FR9913274A FR2799987B1 (fr) 1999-10-25 1999-10-25 Procede d'epuration d'un gaz par adsorption de deux impuretes et dispositif correspondant

Publications (2)

Publication Number Publication Date
EP1095690A1 true EP1095690A1 (de) 2001-05-02
EP1095690B1 EP1095690B1 (de) 2007-04-04

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EP00402895A Expired - Lifetime EP1095690B1 (de) 1999-10-25 2000-10-19 Verfahren zum Reinigen eines Gases und entsprechende Vorrichtung

Country Status (8)

Country Link
US (1) US6319303B1 (de)
EP (1) EP1095690B1 (de)
JP (1) JP2001162126A (de)
AT (1) ATE358524T1 (de)
CA (1) CA2323823C (de)
DE (1) DE60034201T2 (de)
ES (1) ES2283282T3 (de)
FR (1) FR2799987B1 (de)

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CA2323823C (en) 2007-04-10
ATE358524T1 (de) 2007-04-15
JP2001162126A (ja) 2001-06-19
US6319303B1 (en) 2001-11-20
DE60034201T2 (de) 2007-12-20
ES2283282T3 (es) 2007-11-01
FR2799987B1 (fr) 2002-04-26
CA2323823A1 (en) 2001-04-25
FR2799987A1 (fr) 2001-04-27
EP1095690B1 (de) 2007-04-04

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